CN111909505A - Preparation method of reactive flame-retardant sealing material for buildings - Google Patents

Preparation method of reactive flame-retardant sealing material for buildings Download PDF

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CN111909505A
CN111909505A CN202010822141.7A CN202010822141A CN111909505A CN 111909505 A CN111909505 A CN 111909505A CN 202010822141 A CN202010822141 A CN 202010822141A CN 111909505 A CN111909505 A CN 111909505A
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sealing material
parts
component
sulfur
reactive flame
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李荣竹
章丹烽
马红霞
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Dongyang Yan'an Construction Engineering Co ltd
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Dongyang Yan'an Construction Engineering Co ltd
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Abstract

The invention discloses a preparation method of a reactive flame-retardant sealing material for buildings, which comprises the following steps: (1) according to the mass portion, the twoAdding a sulfhydryl monomer, a polyphenol compound, a diisocyanate monomer, a catalyst, a chain extender and an end-capping reagent into a reaction kettle, uniformly stirring at 200-300r/min, introducing nitrogen to displace air in the reaction kettle, and heating to 50-90 DEGoC, reacting for 1.5-3h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane-sulfur rubber liquid; (2) adding a plasticizer, a filler, a coupling agent, a thickening agent and an antioxidant into a reaction kettle, and dispersing for 5-30min at the speed of 2000-3000r/min to obtain a component A of the sealing material; (3) uniformly mixing a vulcanizing agent, a vulcanization accelerator and a plasticizer to obtain a component B of the sealing material; (4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings. The invention obtains the polythiourethane sealing material which has good comprehensive performance and self extinguishes when being away from fire.

Description

Preparation method of reactive flame-retardant sealing material for buildings
Technical Field
The invention relates to the field of high polymer materials, in particular to a preparation method of a reactive flame-retardant sealing material for buildings.
Background
The traditional sealing materials mainly comprise a polyurethane sealing material, a silicone sealing material and a polysulfide sealing material, and the polyurethane sealing material has poor heat resistance, ultraviolet aging resistance and water resistance; the silicone sealing material has good heat resistance, but is not suitable for being used in a completely sealed environment and bonding metals such as copper, brass, magnesium and the like, and has weak bonding strength; the polysulfide glue has better water and oil resistance, but has poor heat resistance and aging resistance. The polythiourethane sealing material is a novel sealing material, overcomes the defects of common strength of silicone sealing materials, easy bubble formation and poor storage stability of the polyurethane sealing materials, and poor long-term durability and deformation displacement resistance of the polythiourethane sealing materials, and has the characteristics of high strength, tear resistance, puncture resistance, good bonding property and the like. The polythiourethane sealing material is a novel adhesive developed on the basis of the traditional adhesive, overcomes some defects of the traditional adhesive, and has good comprehensive performance.
However, polythiourethane sealants have poor flame retardant properties, which limits their use in many applications.
CN201510634891.0 discloses a two-component colorful flexible polythiourethane sealing material and a preparation method thereof. The sealing material consists of a component A and a component B; the component A comprises 15-60 parts by weight of PSU type liquid rubber, 10-30 parts by weight of plasticizer, 10-60 parts by weight of filler, 0.1-5 parts by weight of tackifier, 0.1-5 parts by weight of anti-aging agent and 0.1-5 parts by weight of vulcanization retarder; the component B contains 10-40 parts of vulcanizing agent, 0.1-5 parts of vulcanization accelerator, 10-50 parts of plasticizer, 1-20 parts of colorant and 10-50 parts of filler; the mass ratio of the component A to the component B is 5-15: 1. Grinding the component A and the component B into paste respectively, and then mixing uniformly to obtain the product. The product of the invention has stable storage and excellent physical and mechanical properties, is easy to be prepared into various colors, and overcomes the defect of single color of the existing flexible sealing material.
CN201610540982.2 discloses a polythiourethane/acrylic acid composite hydrogel material, a preparation method and application thereof. The method comprises the following steps: s1, taking DMF as a solvent, reacting a terminal thioglycolic acid low-molecular-weight polyol ester monomer with a diisocyanate monomer to generate polythiourethane, adding HEMA, and reacting to obtain double-bond-terminated polythiourethane; s2, dissolving the double-bond end-capped polythiourethane and an acrylic monomer in DMF (dimethyl formamide), performing ultrasonic treatment to obtain a mixed solution, adding a photoinitiator and a cross-linking agent into the mixed solution, and performing ultrasonic treatment again to obtain a transparent precursor solution; s3, pouring the precursor solution on a polytetrafluoroethylene plate and covering the polytetrafluoroethylene plate with the other plate, and using ultraviolet irradiation to initiate polymerization to obtain the polythiourethane/acrylic acid composite hydrogel material. The composite hydrogel material provided by the invention has high equilibrium water content and high refractive index, and has potential application in the aspect of being used as a lens body material of a soft contact lens or an implant material of a keratoprosthesis.
CN201410292953.X discloses a preparation method of epoxy modified aromatic polythiourethane. The specific operation steps are as follows: reacting liquid polysulfide, macromolecular polyol and isocyanate to synthesize a prepolymer with active hydrogen at the end; reacting epoxy resin with polyisocyanate to generate an isocyanate-terminated adduct; reacting the prepolymer with the addition product to obtain epoxy modified polythiourethane; the small molecular polyamine and the coupling agent form a polyamine curing agent; and (3) mixing the epoxy modified polythiourethane and the polyamine curing agent under the conditions of heating and vacuum, and curing to obtain the epoxy modified aromatic polythiourethane. The hardness is Shore A90-100, and the tensile shear strength is MPa: 8-22, tensile strength MPa: 8-16, air permeability dm 3/min: 0.2-0.5; the composite material is used for paving steel bridge surfaces, and meets the requirements of bonding, high and low temperature resistance, weather resistance, chemical resistance, water seepage resistance and other performances.
In the prior art, the sealing material of polythiourethane is less, and the research on the aspect of flame retardant modification is not involved, so that the application field of the sealing material of polythiourethane is limited, and carbon nanotubes as a filler are easy to agglomerate, so that the defects of poor integral flame retardance and low strength of the material are caused, and the fire risk is brought to the application of the sealing material of polythiourethane as a building.
Disclosure of Invention
The invention provides a preparation method of a reactive flame-retardant building sealing material, and obtains a polythiourethane sealing material which has good comprehensive performance and self extinguishes when being away from fire.
A preparation method of a reactive flame-retardant sealing material for buildings is characterized by comprising the following steps:
(1) according to the mass portion, 25-35 portions of dimercapto monomer, 10-20 portions of polyphenol compound, 15-25 portions of diisocyanate monomer, 0.015-0.05 portion of catalyst, 1-5 portions of chain extender and 1-5 portions of end capping agent are added into a reaction kettle, the mixture is uniformly stirred at 200-300r/min, nitrogen is introduced to displace the air therein, and then the temperature is raised to 50-90 portionsoC, reacting for 1.5-3h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane-sulfur rubber liquid;
(2) adding 5-10 parts of plasticizer, 10-15 parts of amidated sulfur-containing carbon nanotube material, 5-10 parts of coupling agent, 1-5 parts of thickening agent and 0.5-2 parts of antioxidant into a reaction kettle, and dispersing for 5-30min at 3000r/min of 2000-materials to obtain a component A of the sealing material;
(3) uniformly mixing 10-15 parts of vulcanizing agent, 0.1-5 parts of vulcanization accelerator and 10-15 parts of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
Preferably, the dimercaptomonomer in the step (1) is one or a combination of ethylene glycol dimercaptoacetate, bis (mercaptoacetic acid) -1, 4-butylene glycol, dimercaptoethyl sulfide and bis (3-mercaptopropionic acid) ethylene glycol;
preferably, the polyphenol compound in the step (1) is one or a combination of more of 2,2',3,3',5,5',6,6' -octafluoro-4, 4' -bisphenol, hexafluorobisphenol A, tetrabromobisphenol A and bromophenol blue;
preferably, the diisocyanate monomer in step (1) is one or a combination of hexamethylene diisocyanate, 1, 5-naphthalene diisocyanate, biuret triisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate and 2, 4-methyl diisocyanate;
preferably, the catalyst in the step (1) is one or a combination of more of dibutyl dilaurate, stannous oxalate, dimethyl tin dichloride, stannous sulfate, bis (dodecylthio) dibutyl tin and stannous octoate;
preferably, the chain extender in the step (1) is one or a combination of more of 1, 6-hexamethylene diamine, 1, 4-dihydroxy ethoxy benzene, trimethylolpropane, glycerol and butanediamine;
preferably, the end-capping agent in step (1) is one or a combination of isopropanol, n-butanol, tert-butanol, n-pentanol, tert-pentanol and primary pentanol;
the preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 10-20 parts of carboxylated carbon nanotubes in 200 parts of carbon tetrachloride by mass, adding 1.5-3.8 parts of thionyl chloride, controlling the temperature to be 50-70 ℃, stirring for reaction for 2-5h, adding 10-15 parts of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 12-24h, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
Part of reaction mechanism in the preparation process of the reactive flame-retardant building sealing material is shown as follows:
Figure DEST_PATH_IMAGE001
compared with the prior art, the polysulfide polyurethane sealing material which has good comprehensive performance and self extinguishes when being away from fire is obtained. The polythiourethane compound generated by the reaction of the dimercapto monomer, the polyphenol compound and the diisocyanate monomer has rapid crosslinking reaction and can generate a continuous three-dimensional network structure, on the other hand, the addition of the amidated sulfur-containing carbon nanotube material has the synergistic effect with the above to improve the strength, the flame-retardant modification effect is obvious, the oxygen index of the obtained sealing material is 35, the vertical combustion grade is V0 grade, and the tensile strength is 3.5 Mpa.
Drawings
FIG. 1 is a Fourier Infrared Spectroscopy of the product obtained in example 1:
at 2927cm-1The expansion absorption peak of carbon-hydrogen bond nearby is 1732cm-1The absorption peak of carbonyl group of amide at 1375cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, which indicates that hexamethylene diisocyanate participates in the reaction; at 747cm-1The expansion absorption peak of carbon-sulfur bond is present nearby and is 1219cm-1An absorption peak of an ester carbon-oxygen single bond exists nearby, which indicates that the glycol dimercaptoacetate participates in the reaction; at 1476/1375cm-1An absorption peak of benzene ring is present nearby, and is 3304cm-1A stretching absorption peak of phenolic hydroxyl exists nearby, which indicates that 2,2',3,3',5,5',6,6' -octafluoro-4, 4' -bisphenol participates in the reaction; at 683/883cm-1An out-of-plane bending/in-plane bending absorption peak of carbonate ions exists nearby, which indicates that the superfine nano calcium carbonate participates in the reaction; at 1017cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, which indicates that the 1, 6-hexamethylene diamine participates in the reaction.
Detailed Description
The raw materials used in the following examples are all commercially available products, and the examples are further illustrative of the present invention and do not limit the scope of the present invention;
the performance test methods are as follows:
introducing the sealing material into a mould with a corresponding shape, and curing to obtain a sample strip;
1. oxygen index, tested according to astm d 2863;
2. vertical burn rating, tested according to UL 94;
3. tensile strength, tested according to ASTM D638;
example 1
(1) Adding 10g of ethylene glycol dimercaptoacetate, 10g of 2,2',3,3',5,5',6,6' -octafluoro-4, 4' -bisphenol, 15g of hexamethylene diisocyanate, 0.015g of dibutylene dilaurate, 1g of 1, 6-hexamethylene diamine and 1g of isopropanol into a reaction kettle, uniformly stirring at 2000r/min, introducing nitrogen to displace air in the reaction kettle, and then heating to 50 DEGoC, reacting for 1.5h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 5g of plasticizer, 10g of amidated sulfur-containing carbon nanotube material, 5g of coupling agent, 1g of thickening agent and 0.5g of antioxidant into a reaction kettle, and dispersing for 5min at 3000r/min to obtain a component A of the sealing material;
(3) uniformly mixing 10g of vulcanizing agent, 0.1g of vulcanization accelerator and 10g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 10g of carboxylated carbon nanotubes in 100g of carbon tetrachloride, adding 1.5g of thionyl chloride, controlling the temperature to be 50 ℃, stirring and reacting for 2 hours, adding 10g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 12 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 30, a vertical flame rating of V0, and a tensile strength of 3 MPa.
Example 2
(1) Adding 10.6g of bis (mercaptoacetic acid) -1, 4-butylene glycol, 11g of hexafluorobisphenol A, 16.6g of 1, 5-naphthalene diisocyanate, 0.024g of stannous oxalate, 1.6g of 1, 4-dihydroxy ethoxy benzene and 1.6g of n-butyl alcohol into a reaction kettle, stirring uniformly at 2500r/min, introducing nitrogen to displace air in the reaction kettle, and heating to 57 DEGoC, reacting for 1.6h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 5.8g of plasticizer, 10.3g of amidated sulfur-containing carbon nanotube material, 5.8g of coupling agent, 1.3g of thickening agent and 0.7g of antioxidant into a reaction kettle, and dispersing at 2800r/min for 8.7min to obtain a component A of the sealing material;
(3) uniformly mixing 10.7g of vulcanizing agent, 0.4g of vulcanization accelerator and 10.6g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 12g of carboxylated carbon nanotubes in 120g of carbon tetrachloride, adding 1.8g of thionyl chloride, controlling the temperature to be 55 ℃, stirring and reacting for 3 hours, adding 12g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 17 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 31, a vertical burning rating of V0, and a tensile strength of 3.1 MPa.
Example 3
(1) Adding 11.3g of dimercaptoethyl sulfide, 12.3g of tetrabromobisphenol A, 17.8g of biuret triisocyanate, 0.033g of dimethyltin dichloride, 2g of trimethylolpropane and 2.2g of tert-butyl alcohol into a reaction kettle, uniformly stirring at 2800r/min, introducing nitrogen, replacing air in the mixture, and then heating to 60.5 DEGoC, reacting for 1.8h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 6.6g of plasticizer, 11.1g of amidated sulfur-containing carbon nanotube material, 6.2g of coupling agent, 1.7g of thickening agent and 0.8g of antioxidant into a reaction kettle, and dispersing at 2400r/min for 11.5min to obtain a component A of the sealing material;
(3) uniformly mixing 11.3g of vulcanizing agent, 1.1g of vulcanization accelerator and 11.2g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 15g of carboxylated carbon nanotubes in 150g of carbon tetrachloride, adding 2.1g of thionyl chloride, controlling the temperature to be 55 ℃, stirring and reacting for 3 hours, adding 13g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 17 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 31, a vertical burning rating of V0, and a tensile strength of 3.2 MPa.
Example 4
(1) 11.9g of bis (3-mercaptopropionic acid) ethylene glycol, 13.1g of bromophenol blue and 18.4g of isophorone diAdding isocyanate, 0.041g stannous sulfate, 2.6g glycerol and 2.5g n-amyl alcohol into a reaction kettle, uniformly stirring at 2700r/min, introducing nitrogen, displacing air in the reaction kettle, and then heating to 67 DEG CoC, reacting for 1.8h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 7.2g of plasticizer, 11.6g of amidated sulfur-containing carbon nanotube material, 6.8g of coupling agent, 2.3g of thickening agent and 1g of antioxidant into a reaction kettle, and dispersing for 13min at 2500r/min to obtain a component A of the sealing material;
(3) uniformly mixing 11.6g of vulcanizing agent, 1.9g of vulcanization accelerator and 11.9g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 17g of carboxylated carbon nanotubes in 180g of carbon tetrachloride, adding 2.5g of thionyl chloride, controlling the temperature to be 59 ℃, stirring for reaction for 3 hours, adding 14g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, performing reflux reaction for 17 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 31, a vertical burning rating of V0, and a tensile strength of 3.2 MPa.
Example 5
(1) Adding 12.5g of dimercaptoethyl sulfide, 14.2g of hexafluorobisphenol A, 20.1g of diphenylmethane diisocyanate, 0.05g of bis (dodecylthio) dibutyltin, 2.8g of butanediamine and 3.1g of tert-amyl alcohol into a reaction kettle, uniformly stirring at 2600r/min, introducing nitrogen, replacing air in the reaction kettle, and then heating to 70.5oC, reacting for 2 hours, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 7.5g of plasticizer, 12.4g of amidated sulfur-containing carbon nanotube material, 7.6g of coupling agent, 2.7g of thickening agent and 1.1g of antioxidant into a reaction kettle, and dispersing for 16.1min at 2600r/min to obtain a component A of the sealing material;
(3) uniformly mixing 12.2g of a vulcanizing agent, 2.5g of a vulcanization accelerator and 12.5g of a plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 18g of carboxylated carbon nanotubes in 190g of carbon tetrachloride, adding 3.1g of thionyl chloride, controlling the temperature to be 60 ℃, stirring and reacting for 4 hours, adding 14g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 20 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 32, a vertical burning rating of V0, and a tensile strength of 3.2 MPa.
Example 6
(1) Adding 13.1g of bis (mercaptoacetic acid) -1, 4-butylene glycol, 15g of bromophenol blue, 20.8g of 2, 4-methyl diisocyanate, 0.032g of stannous octoate, 3.3g of butanediamine and 3.8g of primary amyl alcohol into a reaction kettle, stirring uniformly at 2200r/min, introducing nitrogen, displacing air in the reaction kettle, and then heating to 75 DEGoC, reacting for 2.1h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 8g of plasticizer, 12.7g of amidated sulfur-containing carbon nanotube material, 7.9g of coupling agent, 3.2g of thickening agent and 1.2g of antioxidant into a reaction kettle, and dispersing for 20.1min at 2200r/min to obtain a component A of the sealing material;
(3) uniformly mixing 12.5g of vulcanizing agent, 2.8g of vulcanization accelerator and 13.1g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 19g of carboxylated carbon nanotubes in 200g of carbon tetrachloride, adding 1.5g of thionyl chloride, controlling the temperature to be 70 ℃, stirring for reaction for 2 hours, adding 15g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, performing reflux reaction for 20 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 33, a vertical burning rating of V0, and a tensile strength of 3.3 MPa.
Example 7
(1) Adding 14.6g of ethylene glycol dimercaptoacetate, 16g of tetrabromobisphenol A, 21.9g of 1, 5-naphthalene diisocyanate, 0.036g of stannous oxalate, 4g of 1, 4-dihydroxy ethoxybenzene and 4.4g of tert-butyl alcohol into a reaction kettle, stirring uniformly at 2200r/min, introducing nitrogen to displace air in the nitrogen, and heating to 78.5oC, reacting for 2.2 hours, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 8.4g of plasticizer, 13.5g of amidated sulfur-containing carbon nanotube material, 8.5g of coupling agent, 3.6g of thickening agent and 1.3g of antioxidant into a reaction kettle, and dispersing for 22.6min at 2100r/min to obtain a component A of the sealing material;
(3) uniformly mixing 12.8g of vulcanizing agent, 3.4g of vulcanization accelerator and 13.6g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 20g of carboxylated carbon nanotubes in 200g of carbon tetrachloride, adding 1.5g of thionyl chloride, controlling the temperature to be 50 ℃, stirring and reacting for 5 hours, adding 15g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 19 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 34, a vertical burning rating of V0, and a tensile strength of 3.4 MPa.
Example 8
(1) Adding 15.9g of bis (3-mercaptopropionic acid) ethylene glycol, 17g of 2,2',3,3',5,5',6,6' -octafluoro-4, 4' -bisphenol, 23.2g of diphenylmethane diisocyanate, 0.045g of dimethyltin dichloride, 4.4g of glycerol and 4.9g of tert-amyl alcohol into a reaction kettle, uniformly stirring at 2400r/min, introducing nitrogen, and placing the mixture in the reaction kettleThe air in the reaction kettle is replaced, and then the temperature is raised to 81.5oC, reacting for 2.4 hours, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 8.7g of plasticizer, 13.8g of amidated sulfur-containing carbon nanotube material, 9.3g of coupling agent, 4.1g of thickening agent and 1.5g of antioxidant into a reaction kettle, and dispersing at 2000r/min for 26.9min to obtain a component A of the sealing material;
(3) uniformly mixing 13.6g of vulcanizing agent, 3.7g of vulcanization accelerator and 14.1g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 20g of carboxylated carbon nanotubes in 200g of carbon tetrachloride, adding 1.5g of thionyl chloride, controlling the temperature to be 50 ℃, stirring and reacting for 5 hours, adding 15g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 24 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 34, a vertical burning rating of V0, and a tensile strength of 3.4 MPa.
Example 9
(1) Adding 20g of bis (mercaptoacetic acid) -1, 4-butylene ester, 20g of tetrabromobisphenol A, 25g of biuret triisocyanate, 0.05g of bis (dodecylthio) dibutyltin, 5g of trimethylolpropane and 5g of isopropanol into a reaction kettle, stirring uniformly at 2500r/min, introducing nitrogen, replacing air in the mixture, and then heating to 90 DEGoC, reacting for 3 hours, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane rubber liquid;
(2) adding 10g of plasticizer, 15g of amidated sulfur-containing carbon nanotube material, 10g of coupling agent, 5g of thickening agent and 2g of antioxidant into a reaction kettle, and dispersing at 2300r/min for 30min to obtain a component A of the sealing material;
(3) uniformly mixing 15g of vulcanizing agent, 5g of vulcanization accelerator and 15g of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
The preparation method of the amidated sulfur-containing carbon nanotube material comprises the following steps:
dispersing 20g of carboxylated carbon nanotubes in 200g of carbon tetrachloride, adding 3.8g of thionyl chloride, controlling the temperature to be 70 ℃, stirring and reacting for 5 hours, adding 15g of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 24 hours, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
The resulting seal material had an oxygen index of 35, a vertical burning rating of V0, and a tensile strength of 3.5 MPa.
Comparative example 1
The number of g of octafluoro-4, 4' -biphenol relative to example 8 was 0g, the oxygen index of the resulting sealing material was 20, the vertical burning rating was V2, and the tensile strength was 3.1 MPa.
Comparative example 2
Relative to example 9, the mass g of amidated sulfur-containing carbon nanotube material was 0g, and the resulting sealing material had an oxygen index of 32, a vertical burning rating of V1, and a tensile strength of 2.6 MPa.
Comparative example 3
In contrast to example 7, tetrabromobisphenol A was replaced with the organophosphate flame retardant, and the resulting sealant had an oxygen index of 25, a vertical burning rating of V1, and a tensile strength of 2.4 MPa.

Claims (8)

1. A preparation method of a reactive flame-retardant sealing material for buildings is characterized by comprising the following steps:
(1) according to the mass portion, 25-35 portions of dimercapto monomer, 10-20 portions of polyphenol compound, 15-25 portions of diisocyanate monomer, 0.015-0.05 portion of catalyst, 1-5 portions of chain extender and 1-5 portions of end capping agent are added into a reaction kettle, the mixture is uniformly stirred at 200-300r/min, nitrogen is introduced to displace the air therein, and then the temperature is raised to 50-90 portionsoC, reacting for 1.5-3h, and cooling to normal temperature to obtain a reactive flame-retardant polyurethane-sulfur rubber liquid;
(2) adding 5-10 parts of plasticizer, 10-15 parts of amidated sulfur-containing carbon nanotube material, 5-10 parts of coupling agent, 1-5 parts of thickening agent and 0.5-2 parts of antioxidant into a reaction kettle, and dispersing for 5-30min at 3000r/min of 2000-materials to obtain a component A of the sealing material;
(3) uniformly mixing 10-15 parts of vulcanizing agent, 0.1-5 parts of vulcanization accelerator and 10-15 parts of plasticizer to obtain a component B of the sealing material;
(4) the component A and the component B are uniformly mixed to obtain the reactive flame-retardant sealing material for buildings.
2. The method according to claim 1, wherein the dimercaptomonomer in step (1) is one or more of glycol dimercaptoacetate, bis (thioglycolic acid) -1, 4-butylene glycol, dimercaptoethyl sulfide, and ethylene glycol bis (3-mercaptopropionate).
3. The method as claimed in claim 1, wherein the polyphenol compound of step (1) is one or more of 2,2',3,3',5,5',6,6' -octafluoro-4, 4' -biphenol, hexafluorobisphenol A, tetrabromobisphenol A, and bromophenol blue.
4. The method according to claim 1, wherein the diisocyanate monomer in step (1) is one or more selected from the group consisting of hexamethylene diisocyanate, 1, 5-naphthalene diisocyanate, biuret triisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, and 2, 4-methyl diisocyanate.
5. The method of claim 1, wherein the catalyst in step (1) is one or more of dibutylene dilaurate, stannous oxalate, dimethyltin dichloride, stannous sulfate, bis (dodecylthio) dibutyltin, and stannous octoate.
6. The method according to claim 1, wherein the chain extender in step (1) is one or a combination of 1, 6-hexanediamine, 1, 4-bis-hydroxyethoxy benzene, trimethylolpropane, glycerol and butanediamine.
7. The method of claim 1, wherein the end-capping reagent in step (1) is one or more selected from isopropanol, n-butanol, t-butanol, n-pentanol, t-pentanol, and primary pentanol.
8. The method of claim 1, wherein the amidated sulfur-containing carbon nanotube material is prepared by:
dispersing 10-20 parts of carboxylated carbon nanotubes in 200 parts of carbon tetrachloride by mass, adding 1.5-3.8 parts of thionyl chloride, controlling the temperature to be 50-70 ℃, stirring for reaction for 2-5h, adding 10-15 parts of 4-dimethylamino thioaniline under the protection of nitrogen, stirring and mixing uniformly, carrying out reflux reaction for 12-24h, filtering after the reaction is finished, and drying to obtain the amidated sulfur-containing carbon nanotube material.
CN202010822141.7A 2020-08-16 2020-08-16 Preparation method of reactive flame-retardant sealing material for buildings Pending CN111909505A (en)

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